Tetrahydrothiophene → HCID 86604150, compound

Participants

Reaction Conditions

Reaction Steps

Tetrahydrothiophene (0.27 mL, 3 mmol) was added to a suspension of compound 24 (200 mg, 0.5 mmol) in dry methanol (5 mL). The solid was dissolved to form a clear solution within 10 min. This solution was filtered via 0.45 μm membrane filter and then heated to 50° C. with stirring for 24 h. After cooling down to room temperature, the solvent was completely removed in vacuo and cold acetone (10 mL) was added to the residue. The precipitate was then filtered and dried to give compound 217a as a colorless, hygroscopic solid (192 mg, 67%): 1H NMR (300 MHz, D2O): 8.17 (2H, s), 4.76 (4H, s), 3.52-3.62 (8H, m), 2.34-2.47 (8H, m); 19F NMR (282 MHz, D2O): −60.2; HR-MS (EI) calcd. for C18H22F6S2Br2 (M+): 573.94, found ([M−Br]+): 495.04.

Provenance & Evidence